p-Fluoronitrobenzene → 1-Ethyl-4-(4-nitrophenyl)piperazine

HRID 13478

Reaktionsgleichung

Reaktionsgleichung von HRID 13478
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[CH2:11]([N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)[CH3:12].C(N(CC)C(C)C)(C)C>CN(C)C=O>[CH2:11]([N:13]1[CH2:18][CH2:17][N:16]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=2)[CH2:15][CH2:14]1)[CH3:12]

Komponenten

5

Edukt 3

HCID 9590p-FluoronitrobenzeneHCID 791961-EthylpiperazineHCID 81531Diisopropylethylamine

Produkt 1

HCID 28575491-Ethyl-4-(4-nitrophenyl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To 4-fluoro-1-nitrobenzene (1 eq) in N,N-dimethylformamide was added Ethyl piperazine (2 eq) and N,N-diisopropylethyl amine (2 eq) and heated at 80° C. for 16 h. Concentrated the resultant mixture and partitioned between ethyl acetate and water. The organic layer was then washed with brine and dried with sodium sulfate and concentrated. Passed through a plug of silica to yield 4-Ethyl-1-(4-nitrophenyl)piperazine. MS: MH+=235.

Aufarbeitung

  1. concentrationConcentrated the resultant mixture
  2. custompartitioned between ethyl acetate and water
  3. washThe organic layer was then washed with brine
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2510e61220fa4f0aa0020614d8a05773
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728010B2

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